Reaktion #623650

ord-7d72175578584c33a4f8163f0c8120b5

Lösungsmittel

Reaktionsbedingungen

Detaillierte Bedingungen
See reaction.notes.procedure_details.

Aufarbeitung

  1. 1
    workup.WAITAfter 3 hours
  2. 2
    Filtrationthe solution was filtered
  3. 3
    Einengenconcentrated
  4. 4
    SonstigeThe resulting residue was purified by silica gel chromatography (gradient elution: 1-15% MeOH/CH2Cl2 with 1% NH4OH)

Vorschrift

To a solution of Example 28A (780 mg, 4.45 mmol) in 7M NH3 in MeOH (5.00 mL) was added to Ra—Ni 2800 water slurry (1.56 g, 26.6 mmol) in a 50 mL pressure bottle. The reaction mixture was and stirred for 10 hours at 30 psi at ambient temperature. After 3 hours, the solution was filtered and concentrated. The resulting residue was purified by silica gel chromatography (gradient elution: 1-15% MeOH/CH2Cl2 with 1% NH4OH) to provide the title compound. MS (DCI+) m/z 182 (M+H)+.

Quelle

DOI: 10.6084/m9.figshare.5104873.v1Patent: US08859584B2uspto-grants-2014_10